4,5-Dichloro-2-nitrophenol → 2-Amino-4,5-dichlorophenol

HRID 588767

反応式

HRID 588767 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([OH:9])=[C:4]([N+:10]([O-])=O)[CH:3]=1>C(O)(=O)C.O.[Fe]>[NH2:10][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([Cl:8])=[CH:6][C:5]=1[OH:9]

参加物

5

反応物 1

HCID 382484,5-Dichloro-2-nitrophenol

生成物 1

HCID 30154152-Amino-4,5-dichlorophenol収率 78%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To a stirred solution of 4,5-dichloro-2-nitrophenol (15 g, 72 mmol) in acetic acid (150 mL) and water (450 mL), iron powder (16 g, 285 mmol) was added in portions. The resulting mixture was stirred at 50° C. for 2 h. The mixture was allowed to cool to room temperature, filtered, and the cake was rinsed with ethyl acetate. The filtrate was extracted with ethyl acetate. The organic layer was washed with water, NaHCO3 (aq.) and brine, dried over Na2SO4 and concentrated in vacuo to afford the desired product (10 g, 78%).

後処理

  1. temperatureto cool to room temperature
  2. filtrationfiltered
  3. washthe cake was rinsed with ethyl acetate
  4. extractionThe filtrate was extracted with ethyl acetate
  5. washThe organic layer was washed with water, NaHCO3 (aq.) and brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bff78745c1124b84b578a242800471d8
出典データセット
uspto-grants-2016_01
特許番号
US09227978B2

関連ノート

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